detection of copper in the synthetic wastewater by using pyrazolidine luminol (pl)

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DETECTION OF COPPER IN THE SYNTHETIC WASTEWATER BY USING PYRAZOLIDINE

LUMINOL (PL)

Syarifah Hikmah Julindaa, Preeda Parkpiana and Srung Smanmoob

aSchool of Environment, Resources and Development, Asian Institute of Technology, 58, Moo 9, km.42, Phaholyothin Highway, Klong Luang, Pathumthani 12120 ThailandbBioresources Research Unit, National Center for Genetic Engineering and Biotechnology (BIOTEC), 113 Thailand Science Park, Phaholyothin Road, Klong 1, Klong Luang, Pathumthani 12120 Thailand

PresentedBy

Syarifah Hikmah Julinda, S.Pi, M.Sc

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Contents

Background of study Research objective Methodology Results and discussions Conclusions

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Media Levels/standard

Seawater <1 µg/ l (Ellingsen et al., 2007)

Lake & river 1-10 µg/ l (Ellingsen et al., 2007)

Drinking water/tap water

< 1300 µg/ l (US EPA, 1993)

Industrial Effluent < 2 mg/l (PCD, 2008)

Environmental levels of Copper

40%

35%

25%

Industrial wastewater

Storm water and surface runoff

Domestic wastewater

Composition of copper releases to water bodies (United States Department of Agriculture, 1998)

Background

Copper is an essential trace elements but also an environmental pollutant

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Measurement

SpectrophotometerSpectrophotometerSample Preparation Method Detection

LimitReference

Acidify with 1:1 HNO3 to pH < 2

AAS 20 µg/litre US EPA (1986)

Filter and acidity sample

ICP 2-10 µg/litre

US EPA (1986)

Filter and acidity sample

ICP-AES 6 µg/litre ATSDR (1990)

Sample solutions should contain 0.5 % HNO3

GF-AAS 1 µg/litre US EPA (1986)

Acid digestion with HNO3, reflux

ICP-MS 0.01 µg/litre

US EPA (1994)

Common methods for Cu (II) ion detection require the use of sophistication and expensive instrumentation

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A dual responsive colorimetric and fluorescent Hg2+ ion from rhodamines based sensor in aqueous media (Huang et al., 2008)

ChemosensorChemosensorUpon binding metals: A fluorescent chemosensor inducesfluorescent change A colorimetric chemosensor exhibitscolor change. This is challengingtechnique since the detection of Cu (II) ion can be achieved by naked eye

Method Detection Limit

Reference

Rhodamine B hydroxylamine as fluorescent chemosensor Cu(II) ion

20 µg/litre

Chen et al (2009)

Terpyridine ascolorimetric chemosensor Hg(II) ion

2 µg/litre

Shunmugam (2008)

Successful chemosensor for detection metals

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Pyrazolidine Luminol (PL)

Cu(II) ionCu(II) ion

Pyrazolidine Luminol Pyrazolidine Luminol

PL is defined as a colorimetric chemosensor for Cu(II) ion detection. Upon binding with Cu(II) ion, PL induces a color change followed by appearing peak of absorbance around 425 nm. (Nasomphan et al., 2009)

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Developing a PL sensor as a colorimetric chemosensor for the detection of Cu (II) ion

Determination of detection limit and optimum conditions of PL sensor

Research objectives

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Methodology

Phase IIDeveloping of

sensor

Phase IPre research

Selectivity of sensor

Detection limit of sensor

Optimum conditions of PL sensor :- Time response - pH

Materials and Reagents Preparation

Synthesis of sensor and 1HNMR analysis

PL sensor solution

Naked eye

UV-vis spectrophotometer

UV-vis spectrophotometer

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PL Cu2+ Ag+ Na+ Mn2+ Zn2+ Co2+ Cd2+ Hg2+ Pb2+ Fe2+ Ba2+ Al2+ Ca2+ Ni2+

Concentration of PL and metal ions were 10-3 M Selectivity of PL sensor

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

Ni2+ Cd2+ Mn2+ Hg2+ Pb2+ Zn2+ Ba2+ Ca2+ Na2+ Ag+ Al2+ Co2+ Fe2+ Cu2+

Metal ions

Abs

425/

350

Absorbance of PL in the presence of various metal ions

Results and discussions

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Detection limit of PL sensor

0 10-3 10-2 10-1 Naked eye :Detection limit found at 3.75 x 10-4 M

UV spectro :Detection limit found at 0.6 x 10-4 M

0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0 2 4 6 8 10 12

Cu(II) ion concentration (mM)

Abso

rban

ce

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Optimum conditions of PL sensor (Cont’)

0.0

0.1

0.2

0.3

0.4

0.5

0 5 10 15 20 30 60

Time (min)

Abso

rban

ce

PL + Cu2+

PL + H2O

0

0.3

0.6

0.9

1.2

0 2 4 6 8 10 12

pH

Abso

rban

ce

Effect of pH on UV-vis results of absorbance PL sensor (10-3 M) at 425 nm upon addition Cu(II) ion 10-3 M

Time influence of UV-vis titration spectra of PL sensor (10-3 M) upon addition Cu(II) ion 10-3 M

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Conclusions There were changes in color of PL sensor upon addition of

Cu(II) ion, followed by appearing peak of absorbance at 425.92 nm (UV-Vis spectra)

Detection limit PL sensor 3.75 x 10-4 M of Cu(II) ion by naked eye observation and 0.6 x 10-4 M by UV-vis spectrophotometer

PL sensor give highly selectivity. In addition, PL sensor was more preferable to Cu(II) ion rather than Cu(I) ion.

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